Hydrochloric Acid → HCID 86674876, compound

HRID 1509342Notes

Reaction equation

HRID 1509342 reaction equation
C([O:7][CH2:8][C:9]([F:15])([F:14])[S:10]([O-:13])(=[O:12])=[O:11])(=O)C(C)(C)C.[C:16]1([I+:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.CO.[OH-].[Na+].Cl>C(Cl)(Cl)Cl>[OH:7][CH2:8][C:9]([F:15])([F:14])[S:10]([O-:13])(=[O:12])=[O:11].[C:23]1([I+:22][C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 86674874HCID 86674874, compound

Product 1

HCID 86674876HCID 86674876, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

In 10 mL of chloroform, 7.32 g of a solid of diphenyliodonium 2-pivaloyloxy-1,1-difluoroethanesulfonate (purity: 90%, equivalent to 13.0 mmol) was dissolved by stirring. The resulting solution was admixed with 26 mL of methanol and 52 mg (1.30 mmol) of sodium hydroxide, and then, reacted at room temperature for 4 hours. To the thus-obtained reaction solution, 0.145 g (1.43 mmol) of concentrated hydrochloric acid was added. The reaction solution was subsequently subjected to concentration under reduced pressure. With this, 5.35 g of the target compound was obtained as a white solid (yield: 97%, purity: 90%).

Workup

  1. customreacted at room temperature for 4 hours
  2. additionwas added
  3. concentrationThe reaction solution was subsequently subjected to concentration under reduced pressure

Sources & evidence

ORD record
ord-6a714f9f0f6d40f6b74a3fed8db32fbc
Source dataset
uspto-grants-2015_12
Patent number
US09221928B2

Reaction notes

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